Process for making phenol



v Sept. .4, 1923.

"Ligg F. COTTRINGER PROCESS FOR MAKING PHENOL Filed April 25., 19.1.8

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Applicatln 186. April, 1918. Serial No. 239,641.

To all 'whom it may'conem: i

Be it known that I, PAUL Gommone, a

'citizen of the `United States, and a resident the principle ofthe -invention being herein explained and the best mode in which I have contemplated applying that principle, so as to distinguish it from other inventions.

The present improvements have more particular. regard to the method of decomposing the phenate and the subsequent recovery of the liberated phenol. One object of the invention accordingly is to provide for the instantaneous removal of the phenol as fast as it is formed from the corresponding phenate. A further object of the invention is to render possible the use of lime instead of caustic. soda in the fusion stage where the phenate is synthetically prepared, instead of being derived from the carbolic acid fraction in coal tar distillation.

To the accomplishment of the `foregoing and'related ends the invention then consists of the steps hereinafter fully described and particularly pointed out in the claims. The annexed drawing and the following description set forth one series of steps for carrying out my improved process, but it will be understood that such steps are merely illusl trative of various ways in which the principle of the invention may be utilized.

The single gure there appearing illus trates in diagrammatic or chart-form, the

- succession of steps involved in carrying out my process. A

Assuming the process to be a synthetic one throughout, calcium benzene-sulphonate is rst made in the usual way, i. e., by neutralizing a mixture of sulphuric and benzene-sulphonic acids by calcium sulphite or carbonate, with the formation of calcium sulphate, calcium benzene-sulphonate, carbon dioxide or .sulphur dioxide xor both, and

water, and if desired, the calcium benzene- -sulphonate may be converted to the correspending sodium salt by treating with sodium carbonate or sulphite.

After obtaining the dry sodium or calcium benzene sulphonate hereinafter'referred to simply as sulphonate, it is placed together Swith from four to seven equivalents of' slaked lime a gasltight rotating drum or cylinder, and the temperature brought up to between 425 C. and 500" C. by external heat applied to such drum; The temperature will have to be considerably higher where the calcium sulphonate is used instead of sodium sulphonate.

After the temperature of the mixture has I been maintained for a short time as described, a current of steam and sulphur dioxide or carbonv dioxide, or else a mixture of all three, is forced through the drum, the interior of which is obviously at a tem.- perature high enough to maintain the steam in a vaporous state. I

After passing through the drum the vapor 1s condensed and the condensate collected in a suitable receptacle. Such condensate will consist of two layers, the upper being a saturated solution of phenol andv water, while the lower heavier layer is a solution Aof water, diphenyl oxide'diphenylene oxide'` and higher vboiling compounds, in phenol. The upper or watery solution of phenol is pumped ort' and boiled, to provide the steam that is mixed with a suitable dioxide in the decomposition step, while the, lower heavier layer is distilled in the usual Way, the first portion of the distillate being put back into the receiver of the drum, and the iinal por- -tion being U. S. P. phenol.

droxy-benzene, ordinarily known as carbol-ic acid (Cel-ISDH), it is to-be understood that this is not by way of limitation, but that the several steps of my improved process are also adaptable to the homologuesl of such phenol, and irrespective of whether it is the monos, or polyhydroxy derivative that is sought.

Other modes of applying the principle of my! invention may be employed instead of the one explained, change being made as re ardethe process herein disclosed, provide the Q j i l incassi step or steps stated by any one 'of the followingl claims or the equivalent of such stated ste or steps be employed.

I there ore particularly point out and dis tinctl claim as my invention 1. gn a method of making phenol, the steps which consist in decomposing with a current of steam and dioxide gas capable or reacting with a phenate a phenate corresponding with the phenol desired, so as to free such phenol; and removing and condensing the resulting vaporv as fast as such phenol is formed.

2. In a method of making phenol, where in a mixture of lime and a sulphonate of the hydrocarbon corresponding with the phenol desired is heated and the corresponding phenate thereby formed; the steps which consist in passing a current of steam and a dioxide gas capable of reacting with a phenate across such mixtureto decompose such phenate and remove the resulting phenol as fast as it is formed; and condensing the resulting vapor and separating the phenol therefrom.

3. In a method of making phenol, the steps which consist in subjecting calcium phenate to a current of steam and a dioxide gas capable of reacting with a phenate to free the phenol; and removing and lcondensing the resulting vapor as fast as such phenol is formed. l 4. ln ay methodl of making phenol, wherein a mixture of a benzene-sulphonate and lime is heated and calciumv phenate there-4 by formed; the steps which consist in passing across such mixture a current of steam and a dioxide gas capable of reacting with a phenate to decompose such phenate and free the phenol, whereby such freed phenol is removed from the other products or such decomposition as fast as it is formed; and condensing the resulting vapor and separating the phenol therefrom.

5. In a method of making phenol, wherein a mixture of a benzene-sulphonate and lime is heated and calcium. phenate thereby formed; the steps which consist in passing across such mixture a current comprising steam and carbon dioxide adapted to decompose such phenate and free the phenol,` whereby such freed phenol is removed from the other products of such decomposition as 4fast as it is formed; and condensing the resulting vapor and separating the phenol therefrom;

6. ln a method of making phenol, wherein a mixture of a benzenesulphonate and lime is heated and calcium phenate thereby formed; the steps which consist in passing a current ofsteam and carbon and sulphur dioxides across such mixture to decompose such phenate and remove the resulting henol as fast as it is formed; and condensing the resulting vapor and separating the phenol therefrom. y

Signed by me, this 19th day of April, 1918.

PAUL corrnrnenn. 

